CN112028623A - Preparation method of heteroatom modified titanate thermistor material - Google Patents

Preparation method of heteroatom modified titanate thermistor material Download PDF

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CN112028623A
CN112028623A CN202010971980.5A CN202010971980A CN112028623A CN 112028623 A CN112028623 A CN 112028623A CN 202010971980 A CN202010971980 A CN 202010971980A CN 112028623 A CN112028623 A CN 112028623A
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temperature
tio
heteroatom
titanate
thermistor material
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季甲
侯银玲
周帆
李远勋
胡安苹
余熙北
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Kaili University
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    • C04B35/634—Polymers
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    • H—ELECTRICITY
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    • H01C—RESISTORS
    • H01C7/00—Non-adjustable resistors formed as one or more layers or coatings; Non-adjustable resistors made from powdered conducting material or powdered semi-conducting material with or without insulating material
    • H01C7/02—Non-adjustable resistors formed as one or more layers or coatings; Non-adjustable resistors made from powdered conducting material or powdered semi-conducting material with or without insulating material having positive temperature coefficient
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Abstract

The invention discloses a preparation method of a heteroatom modified titanate thermistor material. The invention adjusts the temperature rising and falling speed, the highest temperature and the heat preservation time of the sintering furnace; the heating rate used before 800 ℃ is reduced, the binder added during granulation is completely discharged, and the binder which is not discharged is prevented from being carbonized in a ceramic body due to oxygen deficiency to cause pressure resistance reduction; the heating rate after 800 ℃ is increased, the highest sintering temperature is reduced, and abnormal grain growth caused by too slow heating is prevented; the heat preservation time is shortened, so that the porcelain body can be prevented from deforming at high temperature and abnormal growth of crystal grains; the cooling rate is reduced, the crystal grain structure of the product is improved and uniform during cooling, the temperature resistance characteristic of the material is improved, the B value constant of the material is improved, and the voltage resistance Vb is enhanced.

Description

Preparation method of heteroatom modified titanate thermistor material
Technical Field
The invention relates to the technical field of materials, in particular to a preparation method of a heteroatom modified titanate thermistor material.
Background
When the traditional ceramic thermistor PTC element is manufactured again, the BaTiO3 material is generally directly fed, then CaCO3, SrCO3, the donor raw material and the acceptor raw material are added, and the ceramic thermistor PTC element is prepared by ball milling → mixing → granulation, or the BaCO3, SrCO3, CaCO3, the donor raw material and the acceptor raw material are fed together, ball milling → mixing → pre-burning → secondary ball milling → granulation, wherein the ceramic thermistor PTC element prepared by the former process has uneven grain structure, low material B value constant and low voltage resistance Vb; the latter method for preparing the ceramic thermistor PTC element has the disadvantages of complex process, long production period and incapability of timely dealing with orders.
In view of the above, a preparation process of a heteroatom-modified titanate thermistor material is provided for the existing process flow, so as to achieve the purpose of higher economic and practical value.
Disclosure of Invention
The invention aims to provide a preparation method of a heteroatom modified titanate thermistor material, which can solve the problems of uneven crystal grain structure, low material B value constant, low voltage resistance Vb, complex production process, long production period and other adverse factors.
The invention is realized by the following steps: the preparation method of the heteroatom modified titanate thermistor material comprises the following steps:
1) adding trace elements and doped transition elements into a titanate system, carrying out ball milling and mixing, and adding PVA (polyvinyl alcohol) glue for granulation;
2) sintering the ball-milled materials, wherein the temperature reduction rate of the sintering furnace before the temperature is increased to 800 ℃ is 200 ℃/h, after the temperature reaches 800 ℃, the temperature is increased to 1320-.
The titanate system is BaTiO3、CaTiO3And SrTiO3The mass ratio is 70-80: 10-20: 5-15.
The carrier of the trace element is SiO2The carrier doped with transition element is TiO2Wherein, 0.005mol of trace element carrier and 0.03mol of transition element-doped carrier are added into each 1mol of titanate system.
The addition amount of PVA glue is 10-15% of net weight of the material, and the grain size of the granulated material is 150 meshes
The BaTiO3、CaTiO3And SrTiO3Respectively adopting BaCO3With TiO2、CaCO3With TiO2、SrCO3With TiO2Reaction-obtained, reacted BaCO3With TiO2、CaCO3With TiO2、SrCO3With TiO2The molar ratio of (A) to (B) is 1: 1.01-1.03. In the present invention, TiO is added to the system for producing titanate2In excess, eventually in the form of Ti, TiO, in the grain boundaries2The excess can improve the grain structure, and as a result, the withstand voltage can be increased.
If a product with different parameters (such as Curie temperature) is desired, the SrTiO can be adjusted3The amount of (A) changes the Curie temperature and increases SrTiO3In an amount of less BaTiO3By an amount that decreases the curie temperature, and conversely increases the curie temperature.
Due to the adoption of the technical scheme, compared with the prior art, the invention adjusts the temperature rise and fall rate, the highest temperature and the heat preservation time of the nodulizing furnace; the heating rate used before 800 ℃ is reduced, the binder added during granulation is completely discharged, and the binder which is not discharged is prevented from being carbonized in a ceramic body due to oxygen deficiency to cause pressure resistance reduction; the heating rate after 800 ℃ is increased, the highest sintering temperature is reduced, and abnormal grain growth caused by too slow heating is prevented; the heat preservation time is shortened, so that the porcelain body can be prevented from deforming at high temperature and abnormal growth of crystal grains; the cooling rate is reduced, the crystal grain structure of the product is improved and uniform during cooling, the temperature resistance characteristic of the material is improved, the B value constant of the material is improved, and the voltage resistance Vb is enhanced.
Drawings
FIG. 1 is a comparison of the performance of examples of the present invention.
Detailed Description
The embodiment of the invention comprises the following steps: a method for preparing a heteroatom-modified titanate thermistor material, wherein the material to be prepared in this embodiment is a ceramic thermistor (PTC) material with a curie temperature (switching temperature) of 100 ℃, a product size D of 12mm × T of 2.5mm, a resistance of 80 Ω, and a withstand voltage Vb greater than 800V, and the method comprises the following steps:
1) according to the mol ratio of 1: 1.02 preparation of BaCO respectively3And TiO2、CaCO3And TiO2、SrCO3And TiO2After pre-sintering, BaTiO is generated3、CaTiO3、SrTiO3Standby;
2) mixing BaTiO3、CaTiO3And SrTiO3Preparing titanate system according to the ratio of 75: 15: 10, and adding 0.005mol of SiO into each 1mol of titanate system2And 0.03mol of TiO2. Then ball milling and mixing are carried out, and 13 percent of PVA (polyvinyl alcohol) glue is added for granulation;
2) sintering the ball-milled materials, wherein the temperature reduction rate of the sintering furnace before the temperature is increased to 800 ℃ is 200 ℃/h, after the temperature reaches 800 ℃, the temperature is increased to 1320-.
Detecting the obtained product
The experiment takes the example of adding trace elements to improve the pressure resistance:
BaxSr0.08Ca0.12Ti1.01Y0.002 in the original ratio
The prior ratio of BaxSr0.08Ca0.12Ti1.01Y0.002Si0.005
Figure BDA0002684417000000031
Compared with the original proportion, the Vb of R25 (normal temperature resistance value) and the Vb (destruction voltage) are improved by 22.1 percent.

Claims (5)

1. A preparation method of a heteroatom modified titanate thermistor material is characterized by comprising the following steps:
1) adding trace elements and doped transition elements into a titanate system, performing ball milling and mixing, and adding PVA (polyvinyl alcohol) glue for granulation;
2) sintering the ball-milled materials, wherein the temperature reduction rate of the sintering furnace before the temperature is increased to 800 ℃ is 200 ℃/h, after the temperature reaches 800 ℃, the temperature is increased to 1320-.
2. The method for preparing a heteroatom-modified titanate thermistor material according to claim 1, characterized in that: the titanate system is BaTiO3、CaTiO3And SrTiO3The mass ratio is 70-80: 10-20: 5-15.
3. The method for preparing a heteroatom-modified titanate thermistor material according to claim 1, characterized in that: the carrier of the trace element is SiO2The carrier doped with transition element is TiO2Wherein, 0.005mol of trace element carrier and 0.03mol of transition element-doped carrier are added into each 1mol of titanate system.
4. The method for preparing a heteroatom-modified titanate thermistor material according to claim 1, characterized in that: the addition amount of PVA glue is 10-15% of the net weight of the material, and the grain size of the granulated material is 150 meshes.
5. According to claim 1 or2, the preparation method of the heteroatom modified titanate thermistor material is characterized by comprising the following steps: the BaTiO3、CaTiO3And SrTiO3Respectively adopting BaCO3With TiO2、CaCO3With TiO2、SrCO3With TiO2Reaction-obtained, reacted BaCO3With TiO2、CaCO3With TiO2、SrCO3With TiO2The molar ratio of (A) to (B) is 1: 1.01-1.03.
CN202010971980.5A 2020-09-16 2020-09-16 Preparation method of heteroatom modified titanate thermistor material Pending CN112028623A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112608146A (en) * 2020-12-31 2021-04-06 马鞍山巨华电子科技有限公司 Novel environment-friendly PTC thermistor with high-voltage resistance

Citations (4)

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CN103964839A (en) * 2013-01-30 2014-08-06 比亚迪股份有限公司 Positive temperature coefficient thermistor material and its preparation method
CN104311004A (en) * 2014-10-20 2015-01-28 中国科学院上海硅酸盐研究所 PTC ceramic material and method for improving resistance temperature stability below curie point of PTC ceramic material
CN107935587A (en) * 2017-11-18 2018-04-20 四川启兴电子有限公司 A kind of preparation method of lead-free PTC thermal-sensitive electric resistance device

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CN1137679A (en) * 1995-06-02 1996-12-11 上海大地通信电子有限公司 Production process for positive temp. coefficient ceramic thermal resistor
CN103964839A (en) * 2013-01-30 2014-08-06 比亚迪股份有限公司 Positive temperature coefficient thermistor material and its preparation method
CN104311004A (en) * 2014-10-20 2015-01-28 中国科学院上海硅酸盐研究所 PTC ceramic material and method for improving resistance temperature stability below curie point of PTC ceramic material
CN107935587A (en) * 2017-11-18 2018-04-20 四川启兴电子有限公司 A kind of preparation method of lead-free PTC thermal-sensitive electric resistance device

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郑权: "PTC配方与工艺研究", 《中国硕士学位论文全文数据库工程科技I辑》 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112608146A (en) * 2020-12-31 2021-04-06 马鞍山巨华电子科技有限公司 Novel environment-friendly PTC thermistor with high-voltage resistance

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